HRID276761

反应详情

EQUATION

反应方程式

HRID 276761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-tert-Butyl-4-hydroxy-2-furanone (6.6 g, 42 mmol) was dissolved in EtOH (75 mL) with hydrazine hydrate (6.6 mL, 0.21 mol) and was heated at reflux for 16h. The solvent was evaporated and the residue azeotroped with xylene ( 3×50 mL) to afford the title compound (7.2 g, 100%) as a colourless solid. mp 169-172° C. 1H NMR (360 MHz, d6-DMSO) δ1.26 (9H, s), 4.41 (2H, d, J=5.2 Hz), 4.97-5.01 (1H, m), 9.30 (1H, br s), 11.05 (1H, br s). MS (ES+) 171 (M+1).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 16h
  3. customThe solvent was evaporated
  4. customthe residue azeotroped with xylene ( 3×50 mL)